METHOD FOR PRODUCING 3,4-DIHYDRO-1,2,3-OXATHIAZIN-4-ONE-2,2-DIOXIDE COMPOUND OR SALT THEREOF
申请人:Saito Akira
公开号:US20090318685A1
公开(公告)日:2009-12-24
A high quality 3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide compound or a salt thereof is obtained easily and efficiently.
When the compound represented by the following formula (2)
(wherein, R
1
, R
2
, and R
3
are hydrogen atom or an organic group inert to the reaction, and X is hydrogen atom) or a salt thereof is produced by cyclization of a mixture of β-ketoamide-N-sulfonic acid represented by the following formula (1)
or a salt thereof and an inert solvent and a mixture of acid anhydride and an inert solvent, and by subsequent hydrolysis of the product, a step of (A) hydrolyzing the reaction product obtained by the cyclization by mixing with an aqueous solution of sulfuric acid so as a concentration of sulfuric acid in an aqueous phase after the hydrolysis would become 30% by weight or more, and then separating an organic phase and an aqueous phase, or a step of (B) washing the organic phase liquid after the hydrolysis with an aqueous solution of sulfuric acid with a concentration of 30% by weight or more is at least carried out.
可以轻松高效地获得高质量的3,4-二氢-1,2,3-噁嗪-4-酮-2,2-二氧化物化合物或其盐。当通过以下公式(1)所代表的β-酮酰胺-N-磺酸或其盐和惰性溶剂的混合物以及酸酐和惰性溶剂的混合物经环化反应得到以下公式(2)所代表的化合物(其中,R1、R2和R3是氢原子或对反应惰性的有机基团,X是氢原子),并通过随后的水解反应,至少进行以下步骤之一:(A)通过将环化反应所得反应产物与硫酸水溶液混合使得水解后的水相中硫酸的浓度达到30%或更高,然后分离有机相和水相;(B)用30%或更高浓度的硫酸水溶液洗涤水解后的有机相液体。